Page:NIOSH Manual of Analytical Methods - 9111.pdf/2

 METHAMPHETAMINE on Wipes by LC/MS : METHOD 9111, Issue 1, dated 17 October 2011 - Page 2 of 12

REAGENTS: 1.	Methamphetamine.* 1 mg/mL in methanol. (Alltech part # 010013 or equivalent). 2.	Methamphetamine-D14 1 mg/mL in methanol. (Cerilliant part # M-093 or equivalent). 3.	Solvents, residue free analytical grades: a.	 Isopropanol (IPA) * b.	 Acetic Acid * c.	 Acetonitrile * d.	 Methanol * 4.	Concentrated sulfuric acid (AR or trace metals analysis grade).* 5.	Purified gas: nitrogen for drying. 6.	Deionized water (ASTM type II). SOLUTIONS: 1.	Prepare spiking solutions of target analyte and internal standard. Keep solutions refrigerated. Protect solutions from light. a.	 Target analyte spiking solutions are prepared by diluting the 1000 µg/mL methamphetamine stock solution to 200 µg/mL and 20 µg/mL each in methanol. b.	 Dilute 1 mL of 1000 µg/mL methamphetamine-D14 stock solution to 10 mL for a 100 µg/mL (0.1 µg/µL) solution. 2.	Desorption solution: 0.1 M sulfuric acid. Add 22 mL conc. sulfuric acid to 4 L deionized water. 3.	Prepare Mobile Phase A: 0.1% acetic acid, 5% acetonitrile in water. 4.	Prepare Mobile Phase B: 0.1% acetic acid, 95% acetonitrile in water.

EQUIPMENT: 1.	Wipe, cotton gauze, 3” x 3” (7.6 cm x 7.6 cm) 12-ply or 4” x 4” (10.2 cm x 10.2 cm) 8-ply or equivalent. 2.	Sample storage and shipping container: 50-mL polypropylene centrifuge tubes with caps or equivalent. 3.	Liquid chromatograph/mass spectrometer, with integrator or computerized data collection system, and column. 4.	LC autosampler vials, 2-mL, and caps. 5.	Volumetric flasks: various sized flasks for making standards and spiking solutions. A 4-L bottle for making the desorption solution. 6.	Liquid Transfer: a.	 Various microliter syringes for making and spiking standard solutions. b.	 Adjustable 10 to 50-mL desorption solution dispenser to fit 4-L bottle. 7.	Forceps. 8.	Latex or nitrile gloves. Avoid vinyl gloves. (See 9111-3, Sampling, Step 1, NOTE 2.) 9.	Rotating mixer capable of 10-30 rpm. 10.	Pasteur pipettes. 11.	Template: 10 cm x 10 cm hole. Template made of relatively rigid disposable cardstock or sheet of Teflon®. 12.	Filters: Ion Chromatography Acrodisc®, 25 mm syringe filter with 0.45 µm Supor® (PES) membrane. (Pall number 4585T or equivalent). 13.	Ice or other cold media for shipping.

SPECIAL PRECAUTIONS: The solvents are flammable and have associated adverse health effects. Avoid breathing vapors. Avoid skin contact. Work should be performed in an adequate hood. Analysts must wear proper eye and hand protection (e.g. latex gloves) to prevent absorption of even small amounts of amines through the skin as well as for protection from the solvents and other reagents. Dissolving concentrated sulfuric acid in water is highly exothermic. Goggles must be worn. Caution must also be exercised in the handling and analysis of samples. Clandestine drug labs may produce unknown and seriously toxic by-products.
 * See SPECIAL PRECAUTIONS

Method rev. 1.1.1

NIOSH Manual of Analytical Methods (NMAM), Fifth Edition